Synthesis and Characterization of a Calcium-Pyrazolonato Complex. Observation of In-Situ Desolvation During Micro-Electron Diffraction

被引：3

作者：

Mies, Thomas ^{[1
]}

Schurmann, Christian ^{[2
]}

Ito, Sho ^{[3
]}

White, Andrew J. P. ^{[1
]}

Crimmin, Mark R. ^{[1
]}

Barrett, Anthony G. M. ^{[1
]}

机构：

[1] Imperial Coll London, Dept Chem, Mol Sci Res Hub, White City Campus,82 Wood Lane, London W12 0BZ, England

[2] Rigaku Europe SE, Hugenottenallee 167, D-63263 Neu Isenburg, Germany

[3] Rigaku Corp, 3-9-12 Matsubara, Akishima, Tokyo 1968666, Japan

来源：

ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE | 2023年 / 649卷 / 05期

关键词：

SOLVENT-EXTRACTION; ANTITUMOR-ACTIVITY; BETA-DIKETONES; X-RAY; CHEMISTRY; LIGANDS; TAUTOMERISM; LANTHANIDES; DERIVATIVES; SEPARATION;

D O I：

10.1002/zaac.202200294

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

The synthesis and characterization of a calcium pyrazolonato complex is reported. X-ray diffraction (XRD) of single crystals revealed an octahedral geometry with two axial solvent ligands. Analysis of the bulk sample by means of microcrystal electron diffraction (micro-ED) measurement revealed a polymeric pentagonal bipyramidal coordination geometry joined via a central Ca2O2 ring with axial water ligands. During the micro-ED measurement, loss of water was observed resulting in a secondary structure with a polymeric distorted octahedral coordination geometry joined via a central Ca2O2 ring. These findings demonstrate that XRD and micro-ED methods can provide complementary data during structural determination, and that even electrophilic metals are susceptible to desolvation under micro-ED measurements.

引用

页数：7

共 4 条

[1] In-Situ Scanning Electron Microscopy/Electron Backscattered Diffraction Observation of Microstructural Evolution during α → γ Phase Transformation in Deformed Fe-Ni Alloy
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Metallurgical and Materials Transactions A, 2011, 42 : 587 - 593
[2] In-Situ Scanning Electron Microscopy/Electron Backscattered Diffraction Observation of Microstructural Evolution during α → γ Phase Transformation in Deformed Fe-Ni Alloy
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[3] In-situ observation of single-phase compositionally-complex oxide formation during high-pressure and high-temperature synthesis
Yin, Xiaoyu
Xiong, Lianghua
Zhang, Shuya
Chen, Haiyan
Wen, Jianguo
Baldwin, Kenneth
Dong, Anping
Sun, Baode
SCRIPTA MATERIALIA, 2024, 242
[4] IN-SITU OBSERVATION OF SURFACE-MORPHOLOGY EVOLUTION CORRESPONDING TO REFLECTION HIGH-ENERGY ELECTRON-DIFFRACTION OSCILLATION DURING MOLECULAR-BEAM EPITAXY OF GALLIUM-ARSENIDE
HOMMA, Y
OSAKA, J
INOUE, N
JAPANESE JOURNAL OF APPLIED PHYSICS PART 2-LETTERS & EXPRESS LETTERS, 1995, 34 (9B): : L1187 - L1190

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